CN103755691B - The method that Vitexina is extracted from santal leaf - Google Patents
The method that Vitexina is extracted from santal leaf Download PDFInfo
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- CN103755691B CN103755691B CN201410031564.1A CN201410031564A CN103755691B CN 103755691 B CN103755691 B CN 103755691B CN 201410031564 A CN201410031564 A CN 201410031564A CN 103755691 B CN103755691 B CN 103755691B
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- C07—ORGANIC CHEMISTRY
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- C07D407/00—Heterocyclic compounds containing two or more hetero rings, at least one ring having oxygen atoms as the only ring hetero atoms, not provided for by group C07D405/00
- C07D407/02—Heterocyclic compounds containing two or more hetero rings, at least one ring having oxygen atoms as the only ring hetero atoms, not provided for by group C07D405/00 containing two hetero rings
- C07D407/04—Heterocyclic compounds containing two or more hetero rings, at least one ring having oxygen atoms as the only ring hetero atoms, not provided for by group C07D405/00 containing two hetero rings directly linked by a ring-member-to-ring-member bond
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Abstract
The present invention relates to a kind of methods that Vitexina is extracted in leaf from santal, and this approach includes the following steps:(1)Santal leaf is taken, washes, dry, pulverize, then plus methanol solution impregnates, refluxing extraction 1~3 time, merges extracting solution, and filtering obtains filtrate;(2)Filtrate is evaporated, and obtains dry extract, and pH value is adjusted after then adding 50~95 DEG C of hot water to be suspended toward dry extract to acidity;(3)Organic solvent extracts 1~3 time, abandons supernatant, takes middle emulsion layer spare;Lower layer's suspension is ultrasonically treated after determining alcohol is turned up with methanol, is stood, is removed layer and mixed with spare middle emulsion layer containing precipitated liquid;Vacuum filtration;(4)Then it to gained washing of precipitate after suction filtration, then is flowed back and is dissolved with ethanol solution, filtered, recrystallization, then be filtered by vacuum up to Vitexina.This method is simple for process, and production cost is low, obtains the Vitexina that purity is 95% or more, and final Vitexina acquisition amount, which can reach, feeds intake 75% or more of middle Vitexina theoretical content.
Description
Technical field
The present invention relates to the techniques that target component is extracted from plant, and in particular to one kind extracting Vitexina from santal leaf
Method.
Background technology
Santal is sandalwood plants santalSantalum albumL., evergreen dungarunga, it is 6~9 meters high, have parasitic root.Leaf
Ellipticity is oval, film quality, 4-8 centimetres long, 2-4 centimetres wide, the sharp point in top, base portion wedge shape or wealthy wedge shape.
Extraction Vitexina is all to prepare high-end equipment and the fillers such as liquid phase, counter-current chromatograph using preparation, half at present, fixed
Capital input is big, and amount to obtain is only g grades every time, and production technology does not consider cost factor, deducts the life outside fixed assets investment
It produces cost and is far above commodities market price, be unfavorable for industrialized production.
Invention content
To overcome the disadvantages mentioned above and deficiency of prior art, the present invention provides the side that Vitexina is extracted in a kind of leaf from santal
Method.
The method that Vitexina is extracted in a kind of leaf from santal of the present invention, includes the following steps:
(1)Santal leaf is taken, washes, dry, pulverize, then plus methanol solution impregnates, and refluxing extraction 1~3 time merges extraction
Liquid, filtering, obtains filtrate;
(2)Filtrate is evaporated, dry extract is obtained, pH value is adjusted after then adding 50~95 DEG C of hot water to be suspended toward dry extract to acid
Property;
(3)Organic solvent extracts 1~3 time, abandons supernatant, takes middle emulsion layer spare;Lower layer's suspension is turned up with methanol
It is ultrasonically treated after determining alcohol, stands, remove layer and mixed with spare middle emulsion layer containing precipitated liquid, be filtered by vacuum;
(4)Then it to gained washing of precipitate after suction filtration, then is flowed back and is dissolved with ethanol solution, filtered, recrystallization, then vacuum are taken out
It filters up to Vitexina.
Preferably, step(1)The degree of crushing is that can cross 0.5cm*0.5cm~1cm*1cm sieves.
Another preferred embodiment, step(1)The methanol solution is the methanol aqueous solution that volumetric concentration is 50%~90%, is impregnated
When, methanol solution dosage is 5~10 times of santal leaf charged material weight.
Another preferred embodiment, step(1)Temperature is controlled when immersion at 30~60 DEG C, soaking time is 0.5~3h.
Another preferred embodiment, step(1)Each 65~95 DEG C of refluxing extraction temperature.
Another preferred embodiment, step(1)Each reflux extracting time is 0.5~2h.
Another preferred embodiment, step(2)When heating water in toward dry extract, hot water temperature is 70~85 DEG C, and amount of water is every
0.4~1kg dry extracts add water 1L.
Another preferred embodiment, step(2)It is to adjust pH to 1.5~4 that pH, which is adjusted, to acidity.
Another preferred embodiment, step(3)The organic solvent is Ethyl acetate-cyclohexane mixed liquor.Preferably, for the first time
The volume ratio for extracting ethyl acetate and hexamethylene is controlled 20:80~80:20, second extracts ethyl acetate and hexamethylene
Ratio is controlled 100:0~80:20.
Another preferred embodiment, step(3)It is 50%~80% that determining alcohol to volumetric concentration, which is turned up, with methanol, ultrasonic temperature 30~
40 DEG C, ultrasonic 1h rests on 72h at 2~8 DEG C.
Another preferred embodiment, step(4)Washing is equivalent to 4 times of ethyl acetate measured of precipitation volume, 2 times of pure first measured to use
Alcohol, 2 times of water measured wash successively;Ethanol solution is that volumetric concentration is 50% ethanol water.Compared with the prior art, this method
It is more suitable for industrialized production;The extraction separation for the Vitexina that existing achievement in research is previously mentioned is based on laboratory research to obtain
Small quantity sterling(<1g)For the purpose of scientific research, and the production capacity of this method each production cycle reaches kg grades or more;In addition,
This method can be recycled all and be continuing with without great fixed assets investment, organic solvent, compared to existing achievement in research, unit weight
The consumings such as volume production product manpower, the energy, financial resources significantly reduce, and production technology is significantly simplified.
Specific implementation mode
It is exemplified below some currently preferred embodiments of the present invention, with the present invention will be further described, but the implementation of the present invention
Mode is not limited to that.
Embodiment 1
Santal leaf in May newly is adopted, enters net cage on the spot, flowing water washes silt, rack drip-dry aqueous vapor, and the sun is exposed to the sun to dry, powder
It is broken to cross 1cm*1cm steel meshes;Take the broken leaves of 100kg that 70% methanol aqueous solutions of 500L, mixing speed 1 second/turn is added to be impregnated at 40 DEG C
0.5h maintains mixing speed, is heated at reflux to fluidized state, maintains slightly boiling 0.75h, repeat said extracted step 1 time;Merge
Extracting solution is filtered with 20 mesh steel meshes, 200 mesh filter cloth bags, 1000 mesh filter cloth bags, 2000 mesh filter cloth bags, collects filtrate while hot;
It is evaporated with Rotary Evaporators;70 DEG C of hot water 50L are added in dry extract, and ultrasonic agitation presses through 150 mesh steel while hot after being suspended
Sieve, lets cool to room temperature, and pH value is adjusted to 2 with 10% hydrochloric acid;
The pre-saturated Ethyl acetate-cyclohexane of water has been used with pre-prepd(20:80)Mixed solvent 50L acutely shakes extraction
It takes, abandons supernatant;Continue acutely to shake extraction with the pre-saturated ethyl acetate solution 50L of water with pre-prepd, abandons supernatant
Liquid divides and takes middle emulsion layer spare;The pure methanol of 50L is added in lower layer's suspension, and 30 DEG C are ultrasonically treated 1h, stand 72h at 2 DEG C, inhale
It goes supernatant, lower layer to be mixed with spare middle emulsion layer containing precipitated liquid, is filtered by vacuum;
Continue to vacuumize after draining, uses the interior precipitation of 4L ethyl acetate, the pure methanol of 2L, 2L water washings filter successively respectively, often
It is both needed to first drain a solvent before secondary replacement solvent;Precipitation is obtained after washing, it is appropriate to crush, first it is added at one time 50% ethanol water
Solution 3L, after stirring is suspended, heat reflux dissolving such as still has under fluidized state and largely precipitates undissolved, continuously adds 50% ethyl alcohol
Aqueous solution, each 0.5L, until precipitating most of dissolving, until residue precipitation is no longer substantially reduced because of the addition of new soln,
It filters while hot, 72h recrystallizations is stood at 2 DEG C, filter up to the above Vitexina of 95% purity, final Vitexina acquisition amount can reach
Feed intake 75% or more of Vitexina theoretical content.
Embodiment 2:
Santal leaf in June is adopted, enters net cage on the spot, flowing water washes silt, rack drip-dry aqueous vapor, and the sun is exposed to the sun to dry, crushing
Cross 1cm*1cm steel meshes;Take the broken leaves of 100kg that 80% methanol aqueous solutions of 600L, mixing speed 2 seconds/turns is added to impregnate 1h at 45 DEG C, tie up
Mixing speed is held, is heated at reflux to fluidized state, is maintained slightly boiling 1h, repeat said extracted step 1 time;Merge extracting solution, takes advantage of
Hot 20 mesh steel meshes, 200 mesh filter cloth bags, 1000 mesh filter cloth bags, the filtering of 2000 mesh filter cloth bags, collect filtrate, and Rotary Evaporators steam
It is dry;80 DEG C of hot water 40L are added in dry extract, and ultrasonic agitation presses through 150 mesh steel sieve, lets cool to room temperature, with 10% hydrochloric acid while hot after being suspended
PH value is adjusted to 3, the pre-saturated Ethyl acetate-cyclohexane of water has been used with pre-prepd(30:70)Mixed solvent 40L acutely shakes
Extraction is shaken, supernatant is abandoned;Continue to have used the pre-saturated Ethyl acetate-cyclohexane of water with pre-prepd(95:5)Mixed solvent
40L acutely shakes extraction, abandons supernatant, divides and takes middle emulsion layer spare;The pure methanol of 50L, 35 DEG C of ultrasounds are added in lower layer's suspension
1h is handled, 72h is stood at 3 DEG C, sucks supernatant, lower layer mixes containing precipitated liquid with spare middle emulsion layer, is filtered by vacuum, and takes out
Continue to vacuumize after dry, uses the interior precipitation of 4L ethyl acetate, the pure methanol of 2L, 2L water washings filter successively respectively, replace solvent every time
Before be both needed to first drain a solvent;Precipitation is obtained after washing, it is appropriate to crush, it is first added at one time 50% ethanol water 3L, is stirred
After suspension, heat reflux dissolving such as still has under fluidized state and largely precipitates undissolved, continuously adds 50% ethanol water, every time
0.5L, until the most of dissolving of precipitation, residue precipitation filters, 3 DEG C while hot no longer because until the addition of new soln substantially reduces
Lower standing 72h recrystallizations, filter up to the above Vitexina of 95% purity, final Vitexina acquisition amount can reach the middle Vitexina that feeds intake
75% or more of theoretical content.
Embodiment 3:
Santal leaf in July newly is adopted, enters net cage on the spot, flowing water washes silt, rack drip-dry aqueous vapor, and 70 DEG C of air blast electric dry ovens dry
It is dry, it crushed 1cm*1cm steel meshes;Take the broken leaves of 100kg that 90% methanol aqueous solution 700L, mixing speed 3 seconds/turns is added to be impregnated at 50 DEG C
1.5h maintains mixing speed, is heated at reflux to fluidized state, maintains slightly boiling 1.5h, repeat said extracted step 1 time;Merge
Extracting solution is filtered with 20 mesh steel meshes, 200 mesh filter cloth bags, 1000 mesh filter cloth bags, 2000 mesh filter cloth bags while hot, collects filtrate, rotation
Evaporimeter is evaporated;90 DEG C of hot water 30L are added in dry extract, and ultrasonic agitation presses through 150 mesh steel sieve, lets cool to room temperature while hot after being suspended,
PH value is adjusted to 4 with 10% hydrochloric acid, and the pre-saturated Ethyl acetate-cyclohexane of water has been used with pre-prepd(40:60)Mixed solvent
The violent shaking outs of 30L, abandon supernatant;Continue to have used the pre-saturated Ethyl acetate-cyclohexane of water with pre-prepd(90:10)
Mixed solvent 30L acutely shakes extraction, abandons supernatant, divides and takes middle emulsion layer spare;The pure methanol of 50L is added in lower layer's suspension,
40 DEG C are ultrasonically treated 1h, stand 72h at 5 DEG C, suck supernatant, lower layer mixes containing precipitated liquid with spare middle emulsion layer, very
Sky filters, and continues to vacuumize after draining, and uses the interior precipitation of 4L ethyl acetate, the pure methanol of 2L, 2L water washings filter successively respectively, every time
It is both needed to first drain a solvent before replacing solvent;Precipitation is obtained after washing, it is appropriate to crush, it is water-soluble to be first added at one time 50% ethyl alcohol
Liquid 3L, after stirring is suspended, heat reflux dissolving such as still has under fluidized state and largely precipitates undissolved, continuously adds 50% ethanol water
Solution, each 0.5L, until the most of dissolving of precipitation, residue precipitation is taken advantage of no longer because until the addition of new soln substantially reduces
Heat filtering stands 72h recrystallizations at 3 DEG C, filters up to the above Vitexina of 95% purity, final Vitexina acquisition amount can reach throwing
75% or more of Vitexina theoretical content in material.
Embodiment 4:
August santal leaf newly is adopted, enters net cage on the spot, flowing water washes silt, rack drip-dry aqueous vapor, and 70 DEG C of air blast electric dry ovens dry
It is dry, it crushed 1cm*1cm steel meshes;Take the broken leaves of 100kg that pure methanol solution 800L, mixing speed 4 seconds/turns is added to be impregnated at 45 DEG C
1.5h maintains mixing speed, is heated at reflux to fluidized state, maintains slightly boiling 1h, repeat said extracted step 1 time;Merging carries
Liquid is taken, is filtered while hot with 20 mesh steel meshes, 200 mesh filter cloth bags, 1000 mesh filter cloth bags, 2000 mesh filter cloth bags, filtrate is collected, rotation is steamed
Hair instrument is evaporated;95 DEG C of hot water 35L are added in dry extract, and ultrasonic agitation presses through 150 mesh steel sieve while hot after being suspended, let cool to room temperature, use
10% hydrochloric acid adjusts pH value to 3, and the pre-saturated Ethyl acetate-cyclohexane of water has been used with pre-prepd(50:50)Mixed solvent
The violent shaking outs of 35L, abandon supernatant;Continue to have used the pre-saturated Ethyl acetate-cyclohexane of water with pre-prepd(85:15)
Mixed solvent 35L acutely shakes extraction, abandons supernatant, divides and takes middle emulsion layer spare;The pure methanol of 60L is added in lower layer's suspension,
35 DEG C are ultrasonically treated 1h, stand 72h at 6 DEG C, suck supernatant, lower layer mixes containing precipitated liquid with spare middle emulsion layer, very
Sky filters, and continues to vacuumize after draining, and uses the interior precipitation of 4L ethyl acetate, the pure methanol of 2L, 2L water washings filter successively respectively, every time
It is both needed to first drain a solvent before replacing solvent;Precipitation is obtained after washing, it is appropriate to crush, it is water-soluble to be first added at one time 50% ethyl alcohol
Liquid 3L, after stirring is suspended, heat reflux dissolving such as still has under fluidized state and largely precipitates undissolved, continuously adds 50% ethanol water
Solution, each 0.5L, until the most of dissolving of precipitation, residue precipitation is taken advantage of no longer because until the addition of new soln substantially reduces
Heat filtering stands 72h recrystallizations at 3 DEG C, filters up to the above Vitexina of 95% purity, final Vitexina acquisition amount can reach throwing
75% or more of Vitexina theoretical content in material.
Embodiment 5:
(1)September santal leaf newly to be adopted, enters net cage on the spot, flowing water washes silt, rack drip-dry aqueous vapor, and the sun is exposed to the sun to dry,
It crushed 1cm*1cm steel meshes;Take the broken leaves of 100kg that 90% methanol aqueous solutions of 500L, mixing speed 2 seconds/turns is added to be impregnated at 50 DEG C
2h maintains mixing speed, is heated at reflux to fluidized state, maintains slightly boiling 2h, repeat said extracted step 1 time;Merge extraction
Liquid is filtered with 20 mesh steel meshes, 200 mesh filter cloth bags, 1000 mesh filter cloth bags, 2000 mesh filter cloth bags, collects filtrate while hot;
(2)It is evaporated with Rotary Evaporators;90 DEG C of hot water 70L are added in dry extract, and ultrasonic agitation presses through 150 mesh while hot after being suspended
Steel sieves, and lets cool to room temperature, and pH value is adjusted to 3 with 10% hydrochloric acid;
(3)The pre-saturated Ethyl acetate-cyclohexane of water has been used with pre-prepd(20:80)Mixed solvent 50L acutely shakes
Extraction is shaken, supernatant is abandoned;Continue acutely to shake extraction with the pre-saturated ethyl acetate solution 50L of water with pre-prepd, abandon
Supernatant divides and takes middle emulsion layer spare;The pure methanol of 50L is added in lower layer's suspension, and 30 DEG C are ultrasonically treated 1h, are stood at 6 DEG C
72h sucks supernatant, and lower layer mixes containing precipitated liquid with spare middle emulsion layer, vacuum filtration;
(4)Continue to vacuumize after draining, use the interior precipitation of 4L ethyl acetate, the pure methanol of 2L, 2L water washings filter successively respectively,
It is both needed to first drain a solvent before replacing solvent every time;Precipitation is obtained after washing, it is appropriate to crush, first it is added at one time 50% ethyl alcohol
Aqueous solution 3L, after stirring is suspended, heat reflux dissolving such as still has under fluidized state and largely precipitates undissolved, continuously adds 50% second
Alcohol solution, each 0.5L, until the most of dissolving of precipitation, residue precipitation is no longer because the addition of new soln is significantly reduced to
Only, it filters while hot, 72h recrystallizations is stood at 8 DEG C, filter up to the above Vitexina of 95% purity, final Vitexina acquisition amount is reachable
To feeding intake 75% or more of middle Vitexina theoretical content.
Embodiment 6
(1)Newly adopt santal leaf in October, enter net cage on the spot, flowing water washes silt, rack drip-dry aqueous vapor, the sun be exposed to the sun to
It is dry, it crushed 1cm*1cm steel meshes;Take the broken leaves of 100kg that 85% methanol aqueous solutions of 500L, mixing speed 1 second/turn is added to be soaked at 45 DEG C
1h is steeped, mixing speed is maintained, is heated at reflux to fluidized state, is maintained slightly boiling 1h, repeat said extracted step 1 time;Merging carries
Liquid is taken, is filtered while hot with 20 mesh steel meshes, 200 mesh filter cloth bags, 1000 mesh filter cloth bags, 2000 mesh filter cloth bags, collects filtrate;
(2)It is evaporated with Rotary Evaporators;75 DEG C of hot water 50L are added in dry extract, and ultrasonic agitation presses through 150 mesh while hot after being suspended
Steel sieves, and lets cool to room temperature, and pH value is adjusted to 4 with 10% hydrochloric acid;
(3)The pre-saturated Ethyl acetate-cyclohexane of water has been used with pre-prepd(20:80)Mixed solvent 50L acutely shakes
Extraction is shaken, supernatant is abandoned;Continue acutely to shake extraction with the pre-saturated ethyl acetate solution 50L of water with pre-prepd, abandon
Supernatant divides and takes middle emulsion layer spare;The pure methanol of 50L is added in lower layer's suspension, and 30 DEG C are ultrasonically treated 1h, are stood at 4 DEG C
72h sucks supernatant, and lower layer mixes containing precipitated liquid with spare middle emulsion layer, vacuum filtration;
(4)Continue to vacuumize after draining, use the interior precipitation of 4L ethyl acetate, the pure methanol of 2L, 2L water washings filter successively respectively,
It is both needed to first drain a solvent before replacing solvent every time;Precipitation is obtained after washing, it is appropriate to crush, first it is added at one time 50% ethyl alcohol
Aqueous solution 3L, after stirring is suspended, heat reflux dissolving such as still has under fluidized state and largely precipitates undissolved, continuously adds 50% second
Alcohol solution, each 0.5L, until the most of dissolving of precipitation, residue precipitation is no longer because the addition of new soln is significantly reduced to
Only, it filters while hot, 72h recrystallizations is stood at 4 DEG C, filter up to the above Vitexina of 95% purity, final Vitexina acquisition amount is reachable
To feeding intake 75% or more of middle Vitexina theoretical content.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications,
Equivalent substitute mode is should be, is included within the scope of the present invention.
Claims (10)
1. a kind of method for extracting Vitexina in leaf from santal, characterized in that include the following steps:
(1)Santal leaf is taken, washes, dry, pulverize, then plus methanol solution impregnates, and refluxing extraction 1~3 time merges extracting solution,
Filtering, obtains filtrate;
(2)Filtrate is evaporated, dry extract is obtained, pH value is adjusted after then adding 50~95 DEG C of hot water to be suspended toward dry extract to acidity;
(3)Organic solvent extracts 1~3 time, abandons supernatant, takes middle emulsion layer spare;Lower layer's suspension is turned up pure and strong with methanol
It is ultrasonically treated after degree, stands, remove layer and mixed with spare middle emulsion layer containing precipitated liquid, be filtered by vacuum;
(4)Then it to gained washing of precipitate after suction filtration, then is flowed back and is dissolved with ethanol solution, filtered, recrystallization, then be filtered by vacuum i.e.
Obtain Vitexina.
2. the method for extracting Vitexina from santal leaf according to claim 1, characterized in that step(1)The degree of crushing
For 0.5cm*0.5cm~1cm*1cm sieves can be crossed.
3. the method for extracting Vitexina from santal leaf according to claim 1, characterized in that step(1)The methanol is molten
Liquid is the methanol aqueous solution that volumetric concentration is 50%~90%, and when immersion, methanol solution dosage is the 5~10 of santal leaf charged material weight
Times.
4. the method for extracting Vitexina from santal leaf according to claim 1, characterized in that step(1)It is controlled when immersion
For temperature at 30~60 DEG C, soaking time is 0.5~3h.
5. the method for extracting Vitexina from santal leaf according to claim 1, characterized in that step(1)Reflux temperature control
For system at 65~95 DEG C, each reflux extracting time is 0.5~2h.
6. the method for extracting Vitexina from santal leaf according to claim 1, characterized in that step(2)Toward in dry extract
When heating water, hot water temperature is 70~85 DEG C, and amount of water is that every 0.4~1kg dry extracts add water 1L.
7. the method for extracting Vitexina from santal leaf according to claim 1, characterized in that step(2)PH is adjusted to acid
Property for adjust pH to 1.5~4.
8. the method for extracting Vitexina from santal leaf according to claim 1, characterized in that step(3)It is described organic molten
Agent is Ethyl acetate-cyclohexane mixed liquor.
9. the method for extracting Vitexina from santal leaf according to claim 1, characterized in that step(3)It is turned up with methanol
Determining alcohol to volumetric concentration is 50%~80%, and 30~40 DEG C of ultrasonic temperature, ultrasonic 1h rests on 72h at 2~8 DEG C.
10. the method for extracting Vitexina from santal leaf according to claim 1, characterized in that step(4)Washing is to use phase
It is washed successively when in the ethyl acetate of 4 times of amounts of precipitation volume, pure methanol, the 2 times of water measured of 2 times of amounts;Ethanol solution is that volume is dense
Degree is 50% ethanol water.
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Effective date of registration: 20220110 Address after: 510000 room 611, No. 76, yard 12, Jichang Road, Baiyun District, Guangzhou, Guangdong Patentee after: Lin Xiang Address before: 510000 b516, pharmacy building, Guangzhou University of traditional Chinese medicine, No. 232, Waihuan East Road, University City, Panyu District, Guangzhou City, Guangdong Province Patentee before: Lin Li |